气相色谱-质谱法测定水产养殖环境中12种多溴联苯醚  

Determination of 12 Kinds of polybrominated diphenyl ethers in aquaculture environment by gas chromatography-mass spectrometry

作　　者：周明莹[1] 曲克明[1] 马绍赛[1] 陈碧鹃[1] 冷凯良[1] 夏斌[1] 乔向英[1] 

机构地区：[1]中国水产科学研究院黄海水产研究所,农业部海洋渔业资源可持续利用重点开放实验室,山东省渔业资源与生态环境重点实验室,青岛266071

出　　处：《中国渔业质量与标准》2013年第3期64-72,共9页Chinese Fishery Quality and Standards

基　　金："十二五"国家科技支撑计划(2012BAD29B06)

摘　　要：建立了水产养殖环境（水体和沉积物）中BDE-3、BDE-15、BDE-28、BDE-47、BDE-99、BDE-100、BDE-153、BDE-154、BDE-183、BDE-203、BDE-206和BDE-20912种多溴联苯醚同时测定方法。水体样品采用二氯甲烷液-液提取，沉积物样品采用正己烷-丙酮混合溶剂超声提取，提取液用复合硅胶柱净化，用配有EI源的气相色谱-质谱联用仪（GC／MS）测定，内标法定量。结果表明，水体中BDE-3-BDE-206检出限为0．3-5．0ng／L，BDE-209检出限为20．0ng／L，加标回收率为70．8％-114．0％，相对标准偏差为4．1％～10．7％；沉积物中BDE-3～BDE-206检出限为0．05～0．50μg/kg，BDE-209检出限为1．5g/kg，加标回收率为70．4％-116．0％，相对标准偏差为5．9％-12．9％。A gas chromatography- mass spectrometry （GC -MS） method was established for the simultaneous deter- mination of polybrominated diphenyl ethers （PBDEs） in water or sediment. The water samples were extracted by liq- uid - liquid extraction using dichloromethane, meanwhile the sediment samples were extracted by ultrasonic extraction using n - hexane/acetone solution. The samples were purified through multi - layer silica column, The extract cleaned- up was identified and quantified for the 12 PBDEs congeners with internal standard method. According to the vali- dation of the quality control, the results proved that the limit of detection（LOD） in water from BDE -3 to 206 were in the range of 0.3 to 5.0 ng/L, and was 20.0 ng/L for BDE - 209. The recoveries was between 70.8% and 114.0% , and the range of relative standard deviations was from 4.1% to 10.7%. For sediments, the limit of detection（LOD） from BDE - 3 to 206 were in the range of 0.05 to 0.5 μg/kg and was 1.5 μg/kg for BDE - 209. The recoveries were between 70.4% and 116.0%, and the range of relative standard deviations was from 5.9% to 12.9%.

关 键 词：多溴联苯醚 水体 沉积物 气相色谱-质谱 

分 类 号：X832[环境科学与工程—环境工程] O657.63[理学—分析化学]